Since diluting the solution of the calcium salt diminishes its tendency
to form a precipitate with the ammonium acetate the true method of
separation seems to lie in that direction. The calcium salt is held
completely in solution when the separation is made in the following way.
The solution containing the mixed phosphates is diluted so as to
contain not more than one gram thereof in half a liter. To this is
added one drop of dimethylanilin orange, and afterwards ammonium
hydroxid, until a very slight precipitate is formed. The mixture is
heated to 70° and from twenty to twenty-five cubic centimeters of a
twenty-five per cent solution of acid ammonium acetate are added,
enough to change the rose color of the indicator to orange. The iron
aluminum phosphate is separated by filtration and washed with a hot
five per cent solution of ammonium nitrate.
The washed precipitate shows no impurity due to calcium, as proved
by dissolving it, reprecipitating and filtering, adding ammonium
hydroxid to the filtrate, and heating for a long time. Sometimes a
slight troubling of the clear liquid may be observed which may be due
to a slight solubility of the iron aluminum phosphate in washing, an
accident that may occur if the temperature be allowed to fall below
70°, but no weighable amount of material is obtained. If due to
calcium phosphate, a greater dilution in the first precipitation will
remove even this mere trace of that salt. In the above conditions the
contamination of the iron aluminum precipitate with calcium phosphate
may be entirely avoided. We had also undertaken here the problem of
separating the phosphoric acid by the citrate method, followed by a
destruction of the citric acid in the filtrate by combustion with
sulfuric acid according to the kjeldahl process, and final separation
of the iron and alumina in the residues when our attention was called
to substantially the same process as described by Jean.[109] The method
merits a further critical examination.
=126. Phosphoric Acid Soluble in Ammonium Citrate.=—There is no other
point connected with the determination of phosphoric acid which has
excited so much discussion and about which there is such difference of
opinion as the solubility of phosphates in ammonium citrate. It was
clearly established by Huston, in 1882, that the ammonium citrate, as
used in fertilizer analysis, would attack normal tricalcium phosphate
as it exists in bones.[110]
In a raw bone, finely ground, containing 20.28 per cent of phosphoric
acid, the following quantities were found to be soluble in a neutral
ammonium citrate solution of 1.09 specific gravity.
Time of digestion, thirty minutes.
Temperature 30° 40° 50° 60°
Per cent P₂O₅ dissolved 2.76 4.01 3.39 5.88
Public-domain text, read in full here on John Shaqi.
Reviews
Reviews
No reviews yet
Be the first to share your thoughts on this work.
Elsewhere in the archive
Join the Discussion
Join the discussion
Sign in to leave a comment or review.
Sign InorCreate an account